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DILATATION BALLOONS CONTAINING
POLYESTERETHERAMIDE COPOLYMER
Backgrollnd of the Invention
The present invention is generally directed to
dilatation balloons containing polyesteretheramide
copolymer.
The use of balloon catheters ~or coronary
angioplasty is known in the art. In an angioplasty
procedure, a partially occluded blood vessel, i.e., one
containing a stenosis, is treated by the use o~ an
expanding balloon member which presses the stenosis back
against the vessel wall. Typically, the expander member
or balloon is carried on the distal end o~ a dilatation
catheter which is routed through the vascular system to a
locaticn within, for example, a coronary artery
containing a stenotic lesion. Following placement of the
expander member across the lesion as desired, ~luid is
introduced into the proximal end o~ the catheter to
in~late the expander member to a relatively high
pressure, thereby restoring patency to the vessel.
Coronary angioplasty procedures and angioplasty devices
are described in detail in Vliestra et al., "Coronary
Balloon Angioplasty," Blackwell Scientific Publications
(1994).
Medical balloons that are known in the art are
disclosed in the ~ollowing documents: U.S. Patent Nos.
4 964 853 and 4 994 032 to Sugiyama et al; U.S. Patents
No. 4 906 244, 5 108 415, 5 156 612, 5 236 659, and
~ 5 304 197, to Pinchuk et al; U.S. Patent Nos. 5 226 880
30 and 5 334 148 to Martin; U.S. Patent No. 5 250 069 to
CA 022l9744 l997-l0-28
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Nobuyoshi et al; U.S. Patent No. 5,328,468 to Kaneko et
al.; European Patent Application No. 0 566 755; and
Japanese laid-open patent application No. 58-188463.
(All documents cited herein, including the foregoing, are
incorporated herein in their entireties for all
purposes.)
It is an object of the present invention to provide
a balloon for an angioplasty device which is made, at
least in part, of polyesteretheramide copolymer.
Other objects and advantages of the invention will
become apparent to those skilled in the art through
familiarization with the specification and claims herein.
Sllmm~ry of the Invent;on
In sum, the present invention relates to a balloon
for an angioplasty device having a single polymeric
layer. The layer may have from about 20 to about 100
weight pércent polyesteretheramide copolymer and from
about 0 to about 80 wei~ht percent polyamide. The layer
contains substantially no polyetheramide having
substantially no ester linkages. The polyesteretheramide
copolymer may be a block or random copolymer. The
polyesteretheramide copolymer may have a hardness of from
about 45 Shore D to about 78 Shore D, preferably from
about 55 Shore D to about 75 Shore D, and more preferably
~rom about 63 to about 72 Shore D. Even more pre~erably,
the polyesteretheramide copolymer may have a hardness
selected from about 63 Shore D, about 70 Shore D, and
about 72 Shore D. The single polymeric layer may contain
at least about 2 weight percent polyamide such as nylon
12, nylon 11, nylon 6, nylon 6/6, nylon -4/6, and
CA 02219744 1997-10-28
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combinations thereof. The single polymeric layer may
further contain at least about Z wei~ht percent polymer
such as polyester copolymer, polyurethane copolymer,
polyethylene, and combinations thereof. The polymeric
layer may have at least about 40 weight percent
polyesteretheramide copolymer and more preferably at
least about 80 weight percent polyesteretheramide
copolymer. The balloon may have from about 20 to about 80
weight percent nylon 12 and about 20 to about 80 weight
percent polyesteretheramide copolymer, preferably about
60 weight percent nylon 12 and about 40 weight percent
polyesteretheramide copolymer. Alternatively, the balloon
may have about 25 to about 80 weight percent nylon 4/6
and about 20 to about 75 weight percent
polyesteretheramide copolymer, preferably about 65 weight
percent nylon 4/6 and about 35 weight percent
polyesteretheramide copolymer.
The present invention also relates to a balloon for
an angioplasty device having a single polymeric layer
consisting essentially of a polyesteretheramide
copolymer. The polyesteretheramide copolymer may be a
block or random copolymer. The polyesteretheramide
copolymer may have a hardness of from about 45 Shore D to
about 78 Shore D, preferably from about 55 Shore D to
about 75 Shore D, and more preferably about 63 to about
72 Shore D. Even more pre~erably the polyesteretheramide
copolymer may have a hardness selected ~rom 63 Shore D,
70 Shore D, and 72 Shore D. The balloon may consist of
polyesteretheramide.
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The present invention also relates to a balloon for
an angioplasty device having a single polymeric layer
having (a) at least 9l weight percent polyesteretheramide
copolymer, (b) from 0 to 9 weight percent polyamide, and
S (c) from 0 to 9 weight percent of a polymer other than
polyesteretheramide and polyamide. The balloon may have
at least about 95 weight percent polyesteretheramide
copolymer.
Descr;pt;o~ of the ~raw;ngs
FIG. l is a perspective view of an expander member
of the present invention joined to the distal end of a
catheter;
FIG. 2 is a cross-sectional view of a balloon form
used to make expander members of the present invention;
FIG. 3 is a schematic view of a mold apparatus used
to make expander members of the present invention;
FIG. 4 shows a response surface that details the
effects of processing variables and material selection on
balloon wall thickness for PEBAX 6333 balloons;
FIG. 5 shows a response surface that details the
effects of processing variables and material selection on
balloon burst pressure for PEBAX 6333 balloons;
FIG. 6 shows a response surface that details the
effects of processing variables and material selection on
balloon K-stat for PEBAX 6333 balloons;
FIG. 7 shows a response sur~ace that details the
effects of processing variables and material selection on
balloon hoop stress for PEBAX 6333 balloons;
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FIG. 8 shows a response surface that details the
effects of processing variables and material selection on
balloon wall thickness for PEBAX 7033 balloons;
FIG. 9 shows a response surface that details the
effects of processing variables and material selection on
balloon burst pressure for PEBAX 7033 balloons;
FIG. 10 shows a response surface that details the
effects of processing variables and material selection on
balloon K-stat 7033 for PEBAX 7033 balloons.;
FIG. 11 shows a response surface that details the
effects of processing variables and material selection on
balloon hoop stress for PEBAX 7033 balloons;
FIG. 12 shows a response surface that details the
effects of processing variables and material selection on
balloon wall thickness for PEBAX 7233 balloons;
FIG. 13 shows a response surface that details the
effects of processing variables and material selection on
balloon burst pressure for PEBAX 7233 balloons;
FIG. 14 shows a response surface that details the
effects of processing variables and material selection on
balloon K-stat for PEBAX 7233 balloons; and
FIG. 15 shows a response surface that details the
effects of processing variables and material selection on
balloon hoop stress for PEBAX 7233 balloons.
Descript;on of the Preferre~ ~mho~iments
With reference to FIG. 1, expander member 2 is
attached to the distal end of a catheter shaft 4. The
expander member 2, otherwise known as a balloon, has a
single polymeric layer 6 which surrounds the catheter
shaft 4. The expander member 2 shown is bonded at two
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bonding sites 8a,b by thermal bonding, by laser bonding,
with adhesives, or by other methods known in the art.
The expander members o~ the present invention
contain polyesteretheramide copolymer. The structure o~
these polymers consists o~ regular and linear ch~; n~
rigid polyamide blocks and ~lexible polyether blocks.
Such copolymers may be described by the ~ollowing
formula:
O O
HO-~C-PA-C-O-PE-O~iH
where PA is a polyamide block; and
where PE is a polyether block.
Polyesteretheramide copolymer materials are sold
under the trademark PEBAX by Atochem Inc. o~ Glen Rock,
New Jersey. Properties o~ several grades of PEBAX are
disclosed in Atochem's brochure entitled ~'PEBAX Polyether
Block Amide" (December 1987).
The expander member o~ the present invention may
contain polyamide. Polyamide materials include nylon 12,
nylon 11, nylon 6, nylon 6/6, and nylon 4/6. Such
materials are sold under the trademark ZYTEL by Dupont.
The expander member of the present invention may
~urther contain a polymer other than polyesteretheramide
copolymer or polyamide, such as polyester copolymer,
polyurethane copolymer, polyethylene, and combinations
thereo~.
The single polymeric layer making up the expander
member may be a blend o~ suitable materials. Such a
blend may be created by mixing the desired resins and
CA 022l9744 l997-l0-28
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then extruding these resins to form a parison. The
single layer can also be a graft copolymer. Such a graft
copolymer can be ~ormed, ~or example, by reacting
polyamide (such as Nylon 12) with polyphenylether graft
S maleic anhydride (PPE-graft-MA). So called polymer
alloys, and the like, are also included within the
purview of this application.
The expander member of the present invention may be
formed by first generating a parison in an extruder. The
parison will typically have an inside diameter of from
about .01 to .031 inches (0.025 to 0.079 cm), and a wall
thickness of from about .0035 to .015 inches (.0089 to
0.038 cm).
Hot water treated molding devices may then be
utilized to blow mold the expander members of the present
invention. Tubing of the desired material and having a
required size and thickness is inserted into a balloon
processing mold and heated to a temperature of from about
200-212~F (93-100~C). Weight may be added to the mold as
desired. The tubing is subjected to longitll~;n~1 tension
and high-pressure nitrogen 380-500 psi is introduced into
the tubing in the mold. The mold rem~; n.q in a hot water
bath for a predetermined period of time of from about 10-
45 seconds, preferably 25 seconds. The mold is then
removed and placed in a cooling pot for a predetermined
period of time of ~rom about 20-40 seconds, pre~erably 30
seconds, after which the mold may be opened and the
balloon removed.
In an alternative process, the balloons are ~ormed
in balloon blow molding machines. The tubing is inserted
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into the mold and the ends of the tubing secured into
mold gaskets. The tubing is thereafter heated in the
range of 190-220~F (87-104~C) for about 10 to 45 seconds,
preferably 25-30 seconds, and the heated tubing is
subjected to longitll~;n~l tension and expanded 1-2 times
its length in the axial direction. The stretched tubing
is pressurized with nitrogen in the range of about 350-
500 psi and heat treated in the mold for about 10-20
seconds at about 250-280~F (121-138~C), preferably about
260-270~F (127-132~C). The mold is then cooled to room
temperature and allowed to set at room temperature in the
mold under pressure for approximately 10 to 15 seconds.
Thereafter, the system can be depressurized and the
balloon removed from the mold.
~ples
Balloons were made of polyesteretheramide block
copolymer and then tested to determine certain
characteristics.
~x~m~les 1-180
180 balloons were made according to the following
process:
Parisons of 100 weight percent polyesteretheramide
block copolymer were extruded. The parisons had inside
diameters of about .015 inches to about .023 inches, wall
thicknesses of about .006 inches to about .010 inches,
and lengths of about 18 inches.
The parisons were placed in the mold apparatus
illustrated in FIGS. 2 and 3. As shown in FIG. 2, the
balloon form 8 had a void 10 corresponding to the final
shape of the expander member. The void was made up by a
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proximal form 24, a body form 26, and a distal form 28.
With reference to FIG. 3, the distal end of the parison
was inserted into the proximal end 14 of the mold
apparatus 12, and pushed through the proximal form 24,
the body form 26, and the distal form 28 until it exited
the distal end 16 of the mold section. Cap 18 was then
placed over the distal end 16 of the apparatus 12 thereby
clamping and sealing the distal end of the parison. The
mold was then placed in a handle 20 such that the
proximal end of the parison freely extended from the
handle 20. Weights 22 were then placed over the proximal
end of the parison and onto the mold.
The open prox; m~ 1 end of the parison was then
connected to a pressurized nitrogen source by a Touhy
Borst clamp. The nitrogen source was capable of
achieving m~;mllm pressures of 1,000 psi. The nitrogen
source was then opened to varying degrees of between 350-
500 psi and the mold was placed in a bath of hot water
(212~F). The hot water bath warmed the parison. The
freely extending proximal end of the parison was held by
hand such that only about the distal form 28 was under
water, until the mold dropped due to longitudinal
stretching and the distal end of the parison expanded
radially (about 15-30 seconds). Still holding the mold
by hand, the mold continued to drop until it was entirely
under water and the proximal end o~ the balloon expanded
radially (about an additional 1-10 seconds).
The mold was then removed ~rom the hot water bath
and placed in a cold water bath of about 60-75~F ~or
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about 30 seconds. The nitrogen was then shut o~, and
the balloon was removed ~rom the mold.
The balloons were tested by attaching the balloons
to a pressurized nitrogen source in a 37~C water bath,
expanding the balloons under several predetermined
pressures o~ nitrogen (50 psi, 100 psi, 150 psi, and
burst pressure), and then measuring several ~;men~ions
and the burst pressure of the balloons. Dimensions were
measured with a snap gauge.
Tables 1-18 below list certain parameters o~ the
process utilized to make the subject balloons (hot pot
temperature, cold pot temperature, weight added to mold,
and nitrogen pressure). The tables also show results of
the testing o~ the expander members. K stat was
calculated as ~ollows: (Burst pressure)-((K Stat)(Burst
Pressure Standard Deviation)). Hoop stress was calculated
as ~ollows: (Balloon Burst Pressure) (Balloon
Diameter)/(2)(Balloon Wall Thickness).
-
CA 022l9744 l997-l0-28
W 096/37240 PCT/lb9G~_291
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CA 02219744 1997-10-28
W 096/37240 PCTAB96100291
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n ~ O u~ 8 c~ ~ ~ c o o o o o o o o o o O CD m m
1~ 0 ~ I~ ~ ~ ~ ~ ~ ~ ~ o a~, ~
Z ~ n
CA 02219744 1997-10-28
WO 96/37240 PCT~B~G/~291
a~ ~) ~ ~) o o cr) ~ O ~ o "~
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CA 02219744 1997-10-28
W 096/37240 PCTAB9''~291
E, ~ G ~ a ~ ~ S ~ ~
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I O ~ Z ~:
CA 02219744 1997-10-28
W096/37240 PCT/lb9C;~291
a) o ~o ~ o In ~ ~ ~ ~ ~ N
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c o o o O O o ~
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5 (r) 3 ~ O o o o o o o O tD o t
~ T ~ ~ Z ~ ~ tND tD D CnD tD (C~ tD tD 1-- c
CA 02219744 1997-10-28
W 0961372~0 PCT~B96100291
28
E o -' ~ ~ ~ ~ ~ ~ o
_ U~ C o o o o o o o.
C E Q ~~ N N ~ N N
Eo c o o o o o o o
N
,_ O O O O O O ~
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o ul o o o o o o o o o o o
,U C o o o O O ~ ~ ~ o o o ~_
z ~ -
Jo ~n ~ o o o ~ o o o o o o ~ o g
D E ~ c Q~
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o ~ ~ ~ ~ t--'-- ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ -- --
~ ~ I ~_ o ~ ~ ~ ~ ~ ~ ~ 0 0 o ~
~Y~ o o 111 _ ~ ~ m
~ I ~ ~ z ~ ~
CA 02219744 1997-10-28
W096/37240 PCT~B96100291
Examples 181-206
26 balloons were made according to the process
described for Examples 1-180, except that the mold
apparatus did not utilize weights 22 separately, but
S rather incorporated a preselected weight into handle 20.
The balloons were tested to measure distension and
balloon burst strength. Distension is defined as the
ratio of two balloon diameters. In this test, a balloon
was inflated to a series of pressures. The diameter was
measured at each pressure. The distension is the ratio
of the diameter at the lowest pressure to the diameter at
the highest pressure. Inflation was performed at 1 bar
increments up to burst pressure.
To test the balloons, the balloons were first placed
in temperature controlled water bath, and warmed for a
m; n, mllm of 1 minute in water. The balloons were then
attached to a pneumatic inflation/deflation device. A
vacuum was created. Starting with a 4 bar pressure for
20 seconds, the balloon diameter and length were
measured. The balloons were deflated, and the
measurements were recorded. Increasing the pressure by 1
bar, the balloon diameters and lengths were measured.
This procedure was repeated until the balloons bursted.
The burst pressure and the type of burst profile were
recorded.
Tables 19-21 below show the results of the testing
of the expander members.
CA 02219744 1997-10-28
W 096/37240 PCTAB96/00291
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CA 02219744 1997-10-28
W 096/37240 PCT~B96100291
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CA 02219744 1997-10-28
W 096/37240 PCT~B96/00291
~_ CJ) ~ N ~ L~) CD CO O
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O E E E
o X _ _ _
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N N ~ ~ ~
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- ~ x E
a~ ~y x C~ r) ~o SN) tD ~ N Ct) C~
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C Wx
CJ~ CO ~ N ~r LO CD ~ O
--~ co 0 ~ ~ ~ (D ~:~
CA 02219744 1997-10-28
W O 96/37240 PCT~B96/00291
~xamples 207-236
30 balloons were made according to the procedure
described above ~or Examples 1-180, except that parisons
had inside diameters o~ about .025 inches and wall
S thicknesses o~ about .0065 inches.
The balloons were tested according to the procedure
described above ~or Examples 1-180, except that outside
diameters were measured at 1 atm increments from 4-16
atms, and then the balloons were burst.
Tables 22-28 below list certain parameters (PEBAX
grade, dimensions, cone angle, rated burst, and hold time
representing the total amount o~ time that the mold was
held in the water). The tables also show results o~ the
testing o~ the expander members.
CA 02219744 1997-10-28
W 096/37240 PCT~B96/00291
34
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CA 02219744 1997-10-28
W 096/37240 PCT/lb5C/0~291
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CA 02219744 1997-10-28
W 096/37240 PCT~9GJ~291
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W 096/37240 PCT~B96/00291
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CA 02219744 1997-10-28
W096/37240 PCT~B96'~291
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CA 02219744 1997-10-28
W 096/37240 PCTAB96/00291
39
~ N ~'J N ~ N ~ o W
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CA 02219744 1997-10-28
W096/37240 PCT~B96/00291
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F c
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CA 02219744 1997-10-28
W 096/37240 PCTAB9~0~291
~ 4
les 237-266
30 balloons were made according to the procedure
described above for Examples 1-180.
The balloons were tested according to the procedure
described above for Examples 1-180, except that balloons
were tested at 1 atm increments ~rom 4-16 atm and then
burst.
Tables 29-35 below list certain parameters (PEBAX
grade, dimensions, cone angle, rated burst, and hold time
representing the total amount of time that the mold was
held in the water). The tables also show results of the
testing of the expander members.
CA 02219744 1997-10-28
W 096/37240 PCTnB96/00291
42
~ ~, ~ C~l N C~ l N C~ C~ C~ ~ U) o
N ~ ~ ~ ~ N, ~ ~ ~ ~ ~ ~ m N
.~ E
Ir Z a~ ~ ~ ON N ~) N ~ N N ~~ N ~ ~n N
Q ~ m
a~ O C" ~ ON ~ N N N ~ N ~ N C~,~ ~) O (11
O E
J o ~ ~-- t CD ~) O C~ (~ CO O) O N t~ ~~
C~ N cr~ ~n C~ 1 N N N ~I N cr~ tl7 ~ CD ~--
m ~ x ~ Q N ~ ~ ~ ~ ~_ ~ ~ ~ ~ ~ ~ ~ ~ N ~1
~~ ~ O ~-- ~
x ~I) U-) I a~ ~ ~ ~) ~ (~ o ON U ) ~_
. ._ ~ a~ 5
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c~ Cl C_) C~ I m ~
CA 02219744 1997-10-28
W 096/37240 PCT~B9~ 291
': 43
e~ ~ ~ ~ N N N N N N ~ ~ ~ ~ N
N ~ ~ ~ ~, N ' . ~ " ~ ~ ~ ~ ~ N
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X CL ,~ 0 o ~ 0 ~ ~ ~ N N N Q --
., ~ ~ ~
m
- ~ m ~E ~ ~ ~ ~ 0 ~ ~o = N ~ ~ ~ ~ ~ o
1~ (~ Cl~ I m ~
CA 02219744 1997-10-28
W 096/37240 PCTAB96/00291
~ 44
C~ O ~ C~ ~ U~ 1~ CD O ~ ~ 'J O
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CA 02219744 1997-10-28
W O 96/37240 PCTnB96/00291
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07 CO ~r~ C~ N 1~ ~ C~ ~ IS~ O ~ .--
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CA 02219744 1997-10-28
W 096/37240 PCT~B96/00291
46
~t N C~ C0~ ~~ C~ ~ ~
N ~ ~ ~ '-- ~ ~ ~ ~ ~ ~ ~ ~ ~ N
O ~ r-- ~ o c~ c~ 0 ~ ~ ~ ~ O ~
CD ~ ~ ~ N ~1 N N N N N 0 0 0 ~ --
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t~ ~ Z "~ ~ O
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C~ O ~ ~ ~ ~ C~ l C~l N C~ N N 0 0 C'') ~ --
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CA 022l9744 l997-l0-28
W 096/37240 PCT~B96/00291
47
N C~ N ~ ~ N N ~ ~n W
~) O C~ ) O W
C E
~ ~ Z ~t ~ ~ 0 ~ ~ C~ ~ ~ ~t CO W
~I: o
m
~ ~ o ~ ~ u~- 0 o ~ ~ u~ o w
Z
OE a~
O ~D N ~ ) ~ ~ N ~ ~t
~, N ~ Cl ~ ~ ~ ~ ~ N N N N N N ~ ~ C~ u~
. o r~
0 In N L~ c ) ~) O 1~ ~ ~ 0 U) N
n ~ ~ , ~ '6
m ~E ~ ~ ~ ~ ~ ~ o ~ N ~ ~ ~ ~ ~ .~
O W O ~ .--
~ ~ ~ ~ I m ~
CA 02219744 1997-10-28
W 096/37240 PCT~B9C/~8291
48
t~ N ~ N t''J ~ N ~ ~ N ~ . ~ ~ _- O ~ ~ O . ~ ~ ~ ~ t'~l ~ ~ ~ ~ O
t o ~ ~ o ~ ~ o o ~ ~ o o ~ o o ~ o o o o ~ o o o o O O O O O
~ 0
L ~ E
_ y tU tU ~ ~ ~ ~ t~ ~ ~ ~ ~ ~ N t N t~ N t~ N -- ~ t t t t
O ~
c~ C ~ tn (n '~ ~ ~' t'~ tr, t~ t~ t~ t u Itn tU~ 2 tOY~ t~~ t~ t~~, ON O LO ~ ~5) ~ O O O U~ O U~ o
L - o o t~~ t~ ~ o ~ t t~ o ~ t~ ~ ~ t t~ O t~ o o o O o O O O O O O
I_ t t~ O ~ t~J t~ ~ ~n tD ~-- tD t~ O ~ t~ t ~ In tD 1:_ t~) tS~ O ~ t t ~r Ln tD
CA 02219744 1997-10-28
W 096137240 PCTAB96/00291
49
~x~les 267-276
10 balloons were made according to the procedure
described above for Examples 1-180, except that parisons
had inside diameters of about .025 inches and wall
thicknesses of about .0065 inches.
The balloons were tested according to the procedure
described above for Examples 1-180, except that outside
diameters were measured at 1 atm increments from 4-16
atms, and then the balloons were burst.
Tables 36-38 below list certain parameters (PEBAX
grade, dimensions, cone angle, rated burst, and hold time
representing the total amount of time that the mold was
held in the water). The tables also show results of the
testing of the expander members.
CA 02219744 1997-10-28
W 096/37240 PCT/Lbr.~8291
~ ~ ~ CD a~ o ~ ~ ~ ~ ~D ~ ~ cn
a
.C E
z a~ ~ ~ ~ O ~ c~
2 ~_ C C~l ~ ~ ~ ~ ~ ~ ~ C~l ~ ~ C~l N t'~
J O
m
~D ~ 1~
~ z ~D ~ ~ ~ a~ NO N N N N ~ 0 CJ~ N Cl
O E ~
~ O ~ . I_ N (~ ~) O ~ N ~) ~r U) tD 1-- 0 ~ cr) W~ N ~ 0 (D ~ ~ ~ N N N N N N N N N N ~ ~--
m ~ X q~ ~ N ~ ~ ~ ~_ ~ ~ ~ ~ ~ ~ ~ ~ ~ N .
o ~. O l-- ~
-
CJ~ -- ~~ 1~ N U~ ~D ~ O 1-- ~ ~ 0 Lf) N
O ~ ~) ~r CD 1-- CO N N N U~
--.... _ o~ ~ m
0 w ~ ~ F ~ ~ (D ~_ 0 CJ~ ~ ~ N ~ ~ 1~ ~D ~ O
LLI _ O ~ O ~ ._
Q ~ ~ ~ I m~
CA 02219744 1997-10-28
W 096/37240 PCTnB96/00291
~NNNNNNN~ N~
N~'~ N~
-
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C~ llJ O
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W ~ N~NNNNN~N~ ~._
o
O E u~
E a~
o ~ _ N~0NNNNNNNNN~ ~-
m ~ O ~ ~ N~ N~
O . O ~ ~
-
~ ~N~NNN Q_
~ - ~ m ~ E ~ ~ ~ I - ~ ~ o = N~ ~~
I.LI . _ O tll O ~ . ~
~ ~ ~ ~ I m ~
CA 02219744 1997-10-28
W 096/37240 PCTAB9G/~C291
.. o o 8 ~~ 8 8 8 o 8 8
t o ~ ~ ~ ~ ~ ~ o o o
Z~ r l
,~1 LU
~ ~ . tU o~ u~ 8 ~ .~ 8 ~ 8 ~ 8
~ tD O O O O O Q o o o o
a) o n
g Z ~_
CC 1: tl~ ~
m ~ ~ .~ O u~ _ O
LU ' O O O O O O O O O O
l_ tD tD O ~ N t~ ~ U ) tD
N N N N N N N N N N
CA 02219744 1997-10-28
WO 96/37240 PCTAB96/00291
~mrles 277-306
30 balloons were made according to the procedure
described above for Examples 1-180, except that cone
angles were 267 and the parison inside diameter was .025
S inches with a wall thickness of .0065.
The balloons were tested according to the procedure
described above for Examples 1-180, except that outside
diameters were measured at 1 atm increments from 4-16
atms, and then the balloons were burst.
Tables 39-41 below list certain parameters (PEBAX
grade, dimensions, cone angle, rated burst, and hold time
representing the total amount of time that the mold was
held in the water). The tables also show results of the
testing of the expander members.
CA 022l9744 l997-l0-28
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CA 02219744 1997-10-28
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CA 022l9744 l997-l0-28
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F.xi~ es 307-366
60 balloons were made according to the following
procedure: Tubing was placed into a mold and preheated
for 15-30 seconds to a preselected balloon blowing
temperature. The tubing was stretched and inflated to
make a balloon. The balloon was allowed to remain at the
balloon blowing temperature for 15-30 seconds, and then
elevated to at least the crystallization temperature for
10-20 seconds. The balloon was then cooled to room
temperature and removed from the mold.
The balloons were tested according to the procedure
described above for Examples 1-180.
Tables 42-47 below list certain parameters (PEBAX
grade, dimensions, crystallization temperature, mold
temperature, left and right stretch dimensions, nitrogen
pressure, and air flow). The tables also show results of
the testing of the expander members.
CA 022l9744 l997-l0-28
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58
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CA 02219744 1997-10-28
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64
Figures 4-15 were prepared by collecting data
according to material type, and reducing the data to a
series of quadratic equations that include stretch,
crystallization temperature, and balloon blowing
S temperature as dependant variables. The equations were
then plotted using a statistical design of experiments
program called ECHIP . Response variables of interest
were then plotted.
With regard to Figures 4-15, the balloons were
expanded to two times their original length in the axial
direction.
The foregoing specification and figures are
presented for the purpose of illustrating, and not
limiting, the present invention.
